RESUMEN
Objective To develop an HPLC-MS/MS method with solid nuclear particle chromatographic column to determine 15 afrodyn drugs illegally added in sex-enhancing product. Methods The analysis was performed by an HPLC-MS/MS system, with Cortecs-C18 (150 mm × 4.6 mm, 2.7 μm) column. Multiple-reaction monitoring (MRM) was performed to identify and quantify phentolamine mesylate, noracetildenafil, acetildenafil, vardenafil, sildenafil, hydroxyhomosildenafil, homosildenafil, aminotadalafil, tadalafil, thioaildenafil, pseudovardenafil, norneosildenafil, methyltestosterone, stanozolol and danazol, which were extracted with methanol by ultrasonic. Results The linear calibration curves of 15 chemical components mentioned above were obtained at r2 ≥ 0.995 4 with better separation degree and wide linear range. The precision of the method was shown by RSD (n = 6) from six estimated values ranged from 0.9% to 3.3%. The recovery rates determined at three adding concentrations were from 88.3% to 109.5% and the RSD was from 0.9% to 5.2%. The range of limit of quantitation (LOQ) were from 0.015 μg/mL to 0.30 μg/mL and The RSD of inter-day and intra-day precision were from 0.9% to 4.2% and from 1.0% to 4.5%, respectively; Twenty batches of positive samples of 25 batches of sex-enhancing products were detected to be added with sildenafil and with an unqualified rate of 80%. Conclusion The method is specific and simple to detect that 15 afrodyn drugs were added illegally in sex-enhancing product. At the same time, the high positive detection rate should attract the attention of the department concerned, and the corresponding policies should be issued to guarantee the health and safety of the people.
RESUMEN
Novel synthetic analogs of Sildenafil are constantly detected as adulterants in counterfeit drugs and dietary supplements. Their intake constitutes a serious health hazard as side effects are unknown. In this paper an investigation is carried out on NMR and MS/MS spectra of Sildenafil, Thiosildenafil, Acetildenafil and thirteen of their analogs: a list of key signals is reported and discussed with the intent to provide a tool that can help in detecting adulteration and in elucidating the structure of novel analogs. In this view extensive spectral data were reported, discussed and summarized in tables. A discussion on mass fragmentation and NMR chemical shifts is also provided to rationalize assignation. Moreover, a comprehensive information on the route of synthesis is provided for the benefit of those medicines control laboratories that need to synthesize analogs reference standards in-house.